Synthesis Of Series Of Dialkxy Carbamate Quaternary Ammonium Salt Soft Template Agents And Zeolite Molecular Sieve Preparation Research

Template agents were needed in the process of preparation of molecular sieves,which affect with inorganic sources to form regular and orderly micelles assembly,then were removed through calcination,keeping the inorganic framework to obtain molecular sieve.The templates could be divided into hard templates and soft templates.A series of soft templates,series of long chain carbamate quaternary ammonium salt,were designed and synthesized in this dessertation.The synthesis process of these double long chain carbamate quaternary ammonium salts were as follows:the long carbon chain alkyl amine as raw material,dissolved in dichloromethane,reacted with triphosgene to afford long carbon chain isocyanate.Then isocyanates react with 3-dimethylamino-1,2-propylene glycol,using triethylamine as catalyst,to generate intermediate double carbon chain carbamate.Finally,iodomethane as methylating reagent reacted with the above intermediates to obtain the target products.The surface performance of these synthesized carbamate quaternary ammonium salt were measured.Besides,microporous,mesoporous and hierarchical zeolites were prepared in this dissertation to explore the preparation conditions for these synthesized templates to prepare mesoporous molecular sieves.In the isocyanates preparation reaction,the reaction temperature,reaction time should be increased with the growth of carbon chains,which can ensure high yield.While using triethylamine as catalyst in synthesis of carbamates,the reaction conditions,especially the reaction time and the molar ratio of the reactants,should be strictly controlled to minimize the by-products generation.In the process of preparation of the target products,the purity of carbamates must be high enough in order to make the methylation reaction completely,which can finally obtained the target products with high purity.The CMC of lauryl,tetradecyl,hexadecyl and octadecyl carbamate quaternary ammonium salts were 1.56×10-4mol/L,1.35×10-4mol/L,1.22×10-3mol/Land 1.17×10-3mol/L,and the corresponding surface tension of them were 32.26mN/m,36.19mN/m,40.17mN/m and 48.41mN/m,respectively.SEM test were acquired for the prepared microporous,mesoporous and the hierarchical zeolite.The morphology of the microporous molecular sieves was as dispersed block particles,and mesoporous molecular sieves was as a aggregation of spherical particles,while the hierarchical zeolite was as Reunited flaky particles.The intermediate and terminal products were characterized by 1H NMR,13C NMR,HSQC and MS.Microporous,mesoporous and hierarchical zeolites were characterized by XRD and SEM.